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Preparation method of anionic polymerization initiator, device for manufacturing anionic polymerization initiator and anionic polymerization initiator prepared therefrom

a technology anionic polymerization initiator, which is applied in the field of preparation of anionic polymerization initiator, can solve the problems of unstable modification initiator thus prepared, difficult to maintain a constant quality, and low reactivity, so as to prevent instability and inactivation of polymerization initiator and deterioration of physical properties of ssbr, and minimize by-products and unreacted products. , the effect of improving the conversion ra

Active Publication Date: 2019-05-28
LG CHEM LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This approach prevents instability and inactivation of the polymerization initiator, improves the conversion rate, and ensures the production of SSBR with stable and consistent quality, while reducing the reaction time and economic costs associated with batch-wise processes.

Problems solved by technology

However, HMI-Li has a low solubility in a solvent to fall into precipitation over time and also has a problem that the reactivity is lower than that of BuLi, although it can be used as an initiator.
However, the modification initiator thus prepared is unstable over time and falls into precipitation, or is inactivated by bonding a very small amount of oxygen with water.
Therefore, the existing process of preparing the above polymerization initiator in a batch-wise manner and then introducing it into the polymerization reaction necessarily requires a storage step of the modification initiator, thereby bringing about the aforementioned disadvantages.
This may adversely affect the post-processes to be a factor for lowering physical properties of the finally synthesized SSBR, which makes it difficult to maintain a constant quality.
In the case of the former, the storage step of the modification initiator is necessarily required, and during the period of storing the already synthesized initiator its anions are reacted with various scavengers such as moisture and air and thus the initiator loses its activity.
This may adversely affect the post-processes to be a factor for lowering the physical properties of the finally synthesized SSBR, which makes it difficult to maintain a constant quality.
However, it is difficult to confirm whether the modification initiator is properly synthesized, and the physical properties are also deteriorated more than the case of adding the synthesized initiator.
In addition, in all the conventional batch-wise processes, by-products are produced while raw materials are directly introduced, mixed and reacted, or reverse reactions occur to generate unreacted products, and as a result, there is also a problem that a polymerization yield is lowered.

Method used

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  • Preparation method of anionic polymerization initiator, device for manufacturing anionic polymerization initiator and anionic polymerization initiator prepared therefrom
  • Preparation method of anionic polymerization initiator, device for manufacturing anionic polymerization initiator and anionic polymerization initiator prepared therefrom
  • Preparation method of anionic polymerization initiator, device for manufacturing anionic polymerization initiator and anionic polymerization initiator prepared therefrom

Examples

Experimental program
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Effect test

example 1

[0202]Three vacuum-dried stainless steel pressure vessels were prepared. 47 g of hexane, 100 g of 3-vinyl-N,N-dimethylbenzylamine and 101 g of tetramethylethylenediamine were placed in the first pressure vessel to prepare a 3-vinyl-N,N-dimethylbenzylamine solution. Then, 171 g of 2.5M liquid n-butyllithium and 77 g of hexane were placed in another pressure vessel to prepare an n-butyllithium solution.

[0203]The pressure of each pressure vessel was maintained at 4 bar. Then, using a mass flow meter, the 3-vinyl-N,N-dimethylbenzylamine solution was injected into a first inflow line at 0.5 g / min and the n-butyllithium solution was injected into a second inflow line at 0.5 g / min, where each flow meets on a T-union or Y-shaped channel. At this time, the width of the tube or channel was ⅛ inch, the temperature was kept at −30° C., and the internal pressure was maintained at 2 bar using a back pressure regulator. After the two raw materials were mixed, the residence time was adjusted to be ...

example 2

[0204]The anionic polymerization initiator was prepared in the same manner as in Example 1, except that the mixed solution, in which isomers of 2-vinyl-N,N-dimethylbenzylamine, 3-vinyl-N,N-dimethylbenzylamine and 4-vinyl-dimethylbenzylamine were mixed, was used other than the 3-vinyl-N,N-dimethylbenzylamine solution.

example 3

[0205]The anionic polymerization initiator was prepared in the same manner as in Example 1, except that a static mixer other than the tube reactor was used.

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Abstract

A method for preparing an anionic polymerization initiator, a device for manufacturing the same, and an anionic polymerization initiator prepared therefrom is provided. And the method for preparing an anionic polymerization initiator according to the present invention is characterized in that in a continuous reactor an amine compound of Formula 1 and / or Formula 2; an organometallic compound; and / or a conjugated diene compound are introduced in the form of a solution and reacted.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]The present application is a national phase entry under 35 U.S.C. § 371 of International Application No. PCT / KR2016 / 008193 filed Jul. 27, 2016, which claims priority from Korean Patent Application No. 10-2015-0131451 filed Sep. 17, 2015, Korean Patent Application No. 10-2016-0040064 filed Apr. 1, 2016, and Korean Patent Application No. 10-2016-0040066 filed Apr. 1, 2016, all of which are incorporated herein by reference.TECHNICAL FIELD[0002]The present application relates to a method for preparing an anionic polymerization initiator, a device for manufacturing the same, and an anionic polymerization initiator prepared therefrom.BACKGROUND ART[0003]As physical properties of high-efficiency, environment-friendly and high-performance tires are required for reducing discharge of carbon dioxide and improving fuel economy, and the like, tire materials that meet such needs are actively being developed. Particularly, styrene-butadiene rubber obta...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): B60C1/00C08F212/08C07D211/80C07C211/04C08F12/08C08F2/50C08F2/44C08F2/04C08F236/06C07F1/02
CPCC07F1/02B60C1/00C07C211/04C07D211/80C08F2/04C08F2/50C08F12/08C08F212/08C08F236/06C08F2/44B60C1/0016C07C211/27C07D213/24C07D213/53C08F4/48C08F2/06C08F236/10
Inventor CHOE, JAE HOONCHOE, DONG CHEOLKIM, HYUN JUKIM, HYEON HUICHOI, JONG YOUNGLEE, JUNG YONGJEONG, WOONG CHANSHIN, JONG MINKIM, CHAN JOONGSONG, KWANG HO
Owner LG CHEM LTD
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